Apparatus for containing highly corrosive materials under pressure

ABSTRACT

An improved apparatus for containing highly corrosive materials under pressure. The apparatus is utilized in conjunction with a housing having a blind end machined in its bottom and an open end to which a top is connected. The improvement of the present invention comprises means for isolating the corrosive materials to be contained under pressure from the housing and forming a seal having increasing sealing ability in relationship with increasing pressures exhibited in the housing.

United States Patent 91 [111 3,77,421

Brown et al. Dec. 18, 1973 [54] APPARATUS FOR CONTAINING HIGHLY2.547.521 4/195! Buehler 220/3 X CORROSHVE MATERIALS UNDER PRESSUREPrimary Examiner- Herbert F. Ross [75] Inventors: Larry R Brown; VaughanW. Assistant Examiner-Steven M. Pollard Rhoades, both of Tulsa, OklaAtI0rneyJ. Richard Geaman [73] Assignee: Cities Service Oil Company,Tulsa,

Okla [57] ABSTRACT [22] Filed: Oct 22, 1971 An improved apparatus forcontaining highly corrosive materials under pressure. The apparatus isutilized PP 191,663 I in conjunction with a housing having a blind endmachined in its bottom and an open end to which a top is 52 us. ca.220/63, 220/3 connecmd- The improvement of the Present invention 51 Int.Cl B65d 25/14 comprises means isolating the Corrosive materials 58 Fieldof Search 220/63, 64, 3, 46 to be wmained under Pressure from thehousing and forming a seal having increasing sealing ability in rela-[56] References Cited tionship with increasing pressures exhibited inthe UNITED STATES PATENTS 2,647.656 8/1953 Frisch 220/63 R X 3 Claims, 1Drawing Figure \ll'ill'llll llllll'i 8O "|||lll||.ll

/ n(, v 7 s2 at v ' l N "j t N N N 1\ f 2 l8 N t l l APPARATUS FORCONTAINING HIGHLY CORROSIVE MATERKALS UNDER PRESSURE BACKGROUND OF THEINVENTION The present invention relates to means for containing highlycorrosive materials under pressure. More particularly, the apparatus ofthe present invention comprises means for sealing a metallic housingfrom corrosive materials, said means having an increasing ability toseal the housing from the corrosive materials in relationship with anincrease of pressure exhibited by the materials contained within thehousing.

Apparatus utilized for phase equilibria studies, reaction kineticsstudies, reaction of corrosive materials under pressure, and otherphysical and chemical interactions of corrosive materials under pressureand temperature, particularly in the use of high pressure autoclaves,have developed inherent problem wherein the metallic materials ofconstruction utilized for their high strength under pressure forcontaining materials are found to exhibit metallic embrittlement in thepresence of corrosive materials, for example hydrogen sulfide. Thecorrosive effects of the materials contained in the housing weaken themetal, causing disproportionate stresses to develop within the housing,creating a dangerous situation for personnel working within the area ofreaction or experiment.

What is required is apparatus for the containment of highly corrosivematerials under pressure having the conventional form of a housingformed from a metal cylinder and having a blind machined end for abottom and an open end to which a top is connected by two or more boltspassing therethrough and into reamed threaded recesses contained withinthe upper portion of the housing and further having provision for aninlet in the top through which materials may be injected and withdrawn.

It is the object of the present invention to provide apparatus for thecontainment of highly corrosive materials under pressure.

It is a further object of the present invention to provide means forsealing a metallic housing from corrosive materials contained in underpressure so as to prevent metallic embrittlement of the housing.

It is still a further object of the present invention to provideapparatus wherein corrosive materials may be contained under pressurewithin the metallic housing, having appropriate means for sealing thecorrosive materials from the metallic housing, said means exhibiting theability to yield an ever-increasing sealing contact and prevention offluid contact between the corrosive materials and the housing inrelationship with the increasing pressure exhibited by the corrosivematerials contained within the housing.

With these and other objects in mind, the present invention may be morefully understood by referral to the accompanying drawing and thefollowing discussion:

SUMMARY OF THE INVENTION 'The objects of the present invention areaccomplished through utilization of an improved apparatus for containinghighly corrosive materials under pressure. The apparatus forms theconvention configuration of the type comprising a housing formed from ametal cylinder having a blind machined end for a bottom and an open endto which a top is connected by two or more bolts passing therethroughinto reamed and threaded recesses contained within the upper portion ofthe housing and further having an inlet in the top through whichmaterials may be injected or withdrawn. The improvement in the apparatusof the present invention comprises an inert sleeve positioned within thehousing and protecting the metallic housing from the corrosive materialscontained therein. The inert sleeve is utilized in conjunction with alower inertcompressive disc having a diameter approximately that of theinside diameter of the inert sleeve and is positioned in the bottom ofthe housing so as to mate at its sides with the inert sleeve and form aseal against the bottom of the metallic housing, protecting it from thecorrosive materials. A first pressure plate, having a diameter similarto the lower inert-compressive disc, is positioned on the lowerinert-compressive disc within the housing so as to be exposed to thecorrosive materials which are subsequently introduced in the housing. Anupper inert-compressive disc having a diameter approximately of that ofthe inside diameter of the inert sleeve is positioned in the upperportion of the housing so as to mate at its sides with the inert sleeveand form a seal against the top, protecting it from the corrosivematerials. The upper inert compressive-disc has a hole therethrough forthe passage of materials. A second pressure plate, having a diametersimilar to the upper inert-compressive disc, is positioned against theupper inert-compressive disc within the housing and has a hole thereinfor the passage of materials which is aligned with the hole containedwithin the upper inertcompressive disc. In conjunction with the inertsleeve and the upper inert-compressive disc are means for retaining thesecond pressure plate against the upper inert-compressive disc prior topressurization of the corrosive materials within the housing.

BRIEF DESCRIPTION OF THE DRAWING The present invention may be more fullyunderstood by referral to the accompanying drawing in which a housingutilized for pressure studies of highly corrosive materials is depicted,having the improved apparatus of the present invention associatedtherewith.

DETAILED DESCRIPTION OF THE INVENTION The present invention is mosteasily depicted by referral to the accompanying Figure in which theimproved apparatus of the present invention for containing highlycorrosive materials under pressure is depicted. The improved apparatus10 is of the type comprising a housing 12 formed from a metal cylinderhaving a blind machined end 26 thereon for a bottom and an open end towhich a top M is connected by two or more bolts 46 passing therethroughinto reamed threaded recesses 44 contained within the upper portion ofthe housing 12 and further having an inlet 50 in the top 14 throughwhich materials may be injected and withdrawn.

The improvement of the present invention comprises the inert sleeve 16positioned within the housing 12 being formed of an inert material, forexample a rubber such as neoprene, which is inert to corrosive materialsto be studied, for example a hydrogen sulfidehydrocarbon system, therebyprotecting the metallic housing 12 from the corrosive materialscontained within the housing. The lower inert-compressive disc 22 havinga diameter approximately that of the inside diameter of the inert sleeve16 is positioned in the bottom of the housing 26 so as to mate at itssides with the inert sleeve 16 and form a seal against the bottom of themetallic housing 26, protecting it from corrosive materials containedwithin the housing 12. A first pressure plate 18, having a diametersimilar to the lower inert-compressive disc 22 is positioned on thelower inert-compressive disc 22, within the housing 12, so as to beexposed to the corrosive materials subsequently introduced in thehousing 12. An upper inertcompressive disc 24, which also may be formedof an inert-rubber material similar to the material utilized for theinert sleeve 16, having a diameter approximately that of the insidediameter of the inert sleeve 16 is positioned in the top of the housing12 so as to mate at its sides with the inert sleeve 16 and form a sealagainst the top of the metallic housing 14, protecting it from thecorrosive materials. Inert-compressive disc includes a hole 52 forpassage of materials. A second pressure plate 20, having a diametersimilar to the upper inertcompressive disc 24, is positioned against theupper inert compressive disc 24 within the housing 12 so as to beexposed to the corrosive materials contained within the housing 12. Athreaded hole 30 is reamed in the top of the second pressure plate 20for the passage of materials, the hole 30 being aligned with the hole 52in the upper inert-compressive disc which further has an aperture 34aligned with the hole 30 through which materials may pass from withinthe housing to out of the housing.

Means are provided for retaining the second pressure plate 20 againstthe upper inert-compressive disc 24 prior to pressurization of thecorrosive materials within the housing 12. The means may take thepreferred form as shown in the Figure wherein a retaining shaft 28 isprovided having an aperture 36 reamed therethrough in axial alignmentwith its ends and having a diameter such that it may pass through theholes contained within the top of the housing 14 and the upper inertcompressive disc 24 and being threaded on each end with the threads atthe lower end being received by the threads of the second compressiveplate 30. An O-ring 32 is seated in the bottom of the threaded portionof the hole 52 of the second pressure plate 24 so as to form a sealbetween the second pressure plate 24 and the retaining shaft 28.Adjustment nut 40 is turned upon the upper end of the thread 38 of theretaining shaft 28 and backed against the exterior of the top 14 so asto hold the seocnd pressure plate 20 against the upper inert-compressivedisc 24. After loading, the retaining shaft 28 affords upward movementof the plate 20 during fluid pressuring, thereby forming the improvedapparatus for containing highly corrosive materials under pressure ofthe present invention.

Of course, the apparatus of the present invention may take many forms,for example the second pressure plate may be formed of a metallicmaterial with the means for retaining the second pressure plate againstthe upper inert compressive disc comprising magnetic means, for examplean electromagnet 80, externally positioned in proximity to the exteriorof the top so as to draw the pressure plate against the upperinertcompressive disc during the period of loading of the chamber andpressurization of the corrosive materials contained within the chamber.

The materials of construction of the apparatus of the present inventionmay comprise for the housing and top the normal materials utilized forhigh pressure autoclaves utilized in phase equilibria and reactionkinetic studies, for example stainless steel metal alloys. The inertsleeve and inert-compressive discs could comprise, for example rubbercompounds or other materials being non-corrosive to the materialsintroduced within the housing and having a compressibility and cold flowcharacteristic so as to form a seal under pressure. Through theconfiguration of design disclosed herein, the pressure plate maycomprise the same materials of construction as the housing or otherrigid materials which may be subjected to corrosion through extended usein the apparatus of the present invention, but are replaceable and donot form a costly economic deterrant to the fabrication of theapparatus. In a similar fashion, the retaining shaft and bolts maycomprise materials of construction which are not readily corrosive, butgenerally utilized in autoclave design and the O-ring may comprise thesame material as the inert sleeve and inert compressive disc or othermaterials of construction which are not degraded upon exposure to thematerials contained within the housing.

Therefore, the apparatus of the present invention provides means forcontaining highly corrosive materials under pressure through utilizationof sealing means which have the particular ability of forming anincreased sealing capacity upon increase of pressure exhibited withinthe housing. The apparatus removes the inherent problems encountered byprevious high pressure vessels in not requiring expensive materials ofconstruction for the containment of corrosive materials under highpressures and temperatures.

While the invention has been described above with respect to certainembodiments thereof, it will be understood by those skilled in the artthat various changes and modifications may be made without departingfrom the spirit and scope of the invention as set forth herein.

Therefore, we claim:

1. Improved apparatus for containing highly corrosive materials underpressure of the type comprising a housing formed from a metal cylinderhaving a blind machined end for a bottom and an open end to which a topis connected by two or more bolts passing therethrough into reamed andthreaded recesses contained within the upper portion of the housing andfurther having an inlet in the top through which materials may beinjected and withdrawn, the improvement comprising:

a. an inert sleeve positioned within the housing and protecting themetallic housing from the corrosive materials;

b. a lower inert-compressive disc having a diameter approximately thatof the inside diameter of the inert sleeve positioned in the bottom ofthe housing so as to mate at its sides with the inert sleeve and form aseal against the bottom of the metallic housing protecting it from thecorrosive materials;

0. a first pressure plate having a diameter similar to the lowerinert-compressive disc, positioned on the lower inert-compressive discwithin the housing so as to be exposed to the corrosive materialssubsequently introduced in the housing;

d. an upper inert-compressive disc having a diameter approximately thatof the inside diameter of the inert sleeve positioned in the top of thehousing so as to mate at its sides with the inert sleeve and form a sealagainst the top of the metallic housing, prof. means for retaining thesecond pressure plate against the upper inert-compressive disc prior topressurization of the corrosive materials within the housing.

2. The apparatus of claim 1 wherein the second pressure plate hasthreads reamed in the top portion of the hole and the means forretaining the second pressure plate against the upper inert'compressivedisc comprise:

a. a retaining shaft, having an aperture reamed therethrough in axialalignment with its ends and having a diameter such that it may passthrough the holes contained within the top of the housing and the upperinert-compressive disc and being threaded on each end with the threadsof the lower end being received by the threads of the second pressureplate;

b. an O-ring seated in the bottom of the threaded portion of the hole ofthe second pressure plate so as to form a seal between the secondpressure plate and the retaining shaft; and

c. an adjustment nut turned on the upper end of the threads of theretaining shaft and backed against the exterior of the top so as to holdthe second pressure plate against the upper inert-compressive discduring material loading.

3. The apparatus of claim 1 wherein the second pressure plate ismetallic and the means for retaining the second pressure plate againstthe upper inertcompressive disc comprise magnetic means exteriorlypositioned in proximity to the exterior of the top.

1. Improved apparatus for containing highly corrosive materials underpressure of the type comprising a housing formed from a metal cylinderhaving a blind machined end for a bottom and an open end to which a topis connected by two or more bolts passing therethrough into reamed andthreaded recesses contained within the upper portion of the housing andfurther having an inlet in the top through which materials may beinjected and withdrawn, the improvement comprising: a. an inert sleevepositioned within the housing and protecting the metallic housing fromthe corrosive materials; b. a lower inert-compressive disc having adiameter approximately that of the inside diameter of the inert sleevepositioned in the bottom of the housing so as to mate at its sides withthe inert sleeve and form a seal against the bottom of the metallichousing protecting it from the corrosive materials; c. a first pressureplate having a diameter similar to the lower inert-compressive disc,positioned on the lower inertcompressive disc within the housing so asto be exposed to the corrosive materials subsequently introduced in thehousing; d. an upper inert-compressive disc having a diameterapproximately that of the inside diameter of the inert sleeve positionedin the top of the housing so as to mate at its sides with the inertsleeve and form a seal against the top of the metallic housing,protecting it from corrosive materials, and having a hole therethroughfor the passage of materials; e. a second pressure plate having adiameter similar to the upper inert-compressive disc, positioned againstthe upper inert-compressive disc within the housing so as to be exposedto the corrosive materials contained within the housing and having ahole therein for the passage of materials and aligned with the hole inthe upper inert-compressive disc; and f. means for retaining the secondpressure plate against the upper inert-compressive disc prior topressurization of the corrosive materials within the housing.
 2. Theapparatus of claim 1 wherein the second pressure plate has threadsreamed in the top portion of the hole and the means for retaining thesecond pressure plate against the upper inert-compressive disc comprise:a. a retaining shaft, having an aperture reamed therethrough in axialalignment with its ends and having a diameter such that it may passthrough the holes contained within the top of the housing and the upperinert-compressive disc and being threaded on each end with the threadsof the lower end being received by the threads of the second pressureplate; b. an O-ring seated in the bottom of the threaded portion of thehole of the second pressure plate so as to form a seal between thesecond pressure plate and the retaining shaft; and c. an adjustment nutturned on the upper end of the threads of the retaining shaft and backedagainst the exterior of the top so as to hold the second pressuRe plateagainst the upper inert-compressive disc during material loading.
 3. Theapparatus of claim 1 wherein the second pressure plate is metallic andthe means for retaining the second pressure plate against the upperinert-compressive disc comprise magnetic means exteriorly positioned inproximity to the exterior of the top.